NANO EXPRESS Open Access

Pt-decorated nanoporous gold for glucoseelectrooxidation in neutral and alkaline solutionsXiuling Yan1,2*, Xingbo Ge1 and Songzhi Cui1

Abstract

Exploiting electrocatalysts with high activity for glucose oxidation is of central importance for practical applicationssuch as glucose fuel cell. Pt-decorated nanoporous gold (NPG-Pt), created by depositing a thin layer of Pt on NPGsurface, was proposed as an active electrode for glucose electrooxidation in neutral and alkaline solutions. Thestructure and surface properties of NPG-Pt were characterized by scanning electron microscopy (SEM), transmissionelectron microscopy (TEM), X-ray powder diffraction (XRD), and cyclic voltammetry (CV). The electrocatalytic activitytoward glucose oxidation in neutral and alkaline solutions was evaluated, which was found to depend strongly onthe surface structure of NPG-Pt. A direct glucose fuel cell (DGFC) was performed based on the novel membraneelectrode materials. With a low precious metal load of less than 0.3 mg cm-2 Au and 60 μg cm-2 Pt in anode andcommercial Pt/C in cathode, the performance of DGFC in alkaline is much better than that in neutral condition.

IntroductionGlucose is widely used in modern life and industry as anontoxic, inexpensive, and renewable resource. SinceRao and Drake [1] first reported the glucose oxidationon platinized-Pt electrodes in phosphate buffer solutionin the 1960s, electrocatalytic oxidation of glucose hasbeen extensively investigated as a key reaction in thefields of sensors [2,3] and fuel cells [4,5]. Great effortshave been made to develop catalytically active electrodematerials for this reaction in the past two decades. Asone of the most studied electrocatalyst, Pt was found toexhibit considerable activity for glucose oxidation at anegative potential in neutral and alkaline solutions [6].However, systematical study showed that this electroca-talytic process was subject to serious poisoning due toadsorbed intermediates from the oxidation of glucose[7]. To mitigate the poisoning effect, Pt-based bimetalliccatalysts such as Pt-Pb [8,9], Pt-Ru [10,11], and Pt-Au[4,12], have been developed to improve the electrocata-lytic activity and selectivity. On the other hand, it isincreasingly realized that glucose electrooxidation is sen-sitive to surface structure of the electrocatalyst. Forexample, Adzic et al. found that this reaction stronglydepended on the crystallographic orientation of the Pt

electrode surface [13]. Thus, significant attention hasbeen focused on exploiting the potential applications ofthe nanostructured materials with special surface prop-erties for glucose oxidation. Besides the widely usednanoparticles [14,15], many other nanostructures werealso studied, such as carbon nanotubes [16], ordered Ptnanotube arrays [17], mesoporous Pt electrodes [18],and nanoporous Pt-Pb and Pt-Ir networks [8,19]. Whilethese unique nanostructures exhibited considerableadvantages as compared to traditional electrodes, theywere mainly employed for glucose electrochemicaldetection. Exploiting nanostructures for potential appli-cations in glucose fuel cell is still highly desirable.Recently, Erlebacher and co-workers reported an

interesting type of membrane electrode materials callednanoporous gold (NPG) leaves which could be made bychemically etching the white gold (AgAu alloy) leaves incorrosive medium [20]. Coupled with surface functiona-lization with other catalytically active material, such asPt, the 100-nm-thick high surface area electrode materi-als demonstrated superior activities toward a series ofimportant electrochemical reaction including methanoloxidation [21,22] and formic acid oxidation [23]. Preli-minary studies also proved they could work as promis-ing electrocatalysts in proton exchange membrane fuelcells at ultra-low Pt loading [24,25]. Here, we focus ontheir electrocatalytic properties toward glucose oxidationand its application in alkaline glucose fuel cells.

* Correspondence: xiuling1212@gmail.com1School of Chemistry and Chemical Engineering, Shandong University, Jinan250100, China.Full list of author information is available at the end of the article

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© 2011 Yan et al; licensee Springer. This is an Open Access article distributed under the terms of the Creative Commons AttributionLicense (http://creativecommons.org/licenses/by/2.0), which permits unrestricted use, distribution, and reproduction in any medium,provided the original work is properly cited.

ExperimentalReagents and apparatusAll chemicals were of analytical grade and used as pur-chased without further purification. D-Glucose, NaOH,HNO3 (65%), Na2HPO4·12H2O, NaH2PO4·2H2O, andH2PtCl6·6H2O were obtained from Sinopharm ChemicalReagent Co., Ltd. Au/Ag alloy (50:50, wt%) leaves withthickness of 100 nm (Sepp Leaf Products, New York)were used for NPG fabrication. Ultrapure water(18.2 MΩ) was used throughout the experiments and0.1 M PBS was prepared with pH 7.4. The compositionof NPG-Pt sample was determined by an IRIS Advan-tage inductively coupled plasma-atomic emission spec-trometry (ICP-AES). The surface structure of NPG-Ptwas observed JSM-6700F SEM and JEM-2100 TEM. Thecrystallographic information was obtained with XRD(Bruker D8 Advance X-ray diffractometer, Cu Ka radia-tion l = 1.5418 Å) at a 0.02°/s scan rate. All electroche-mical measurements were performed at room temperatein a traditional three-electrode electrochemical cell witha CHI 760C electrochemical workstation (Shanghai).Mercury sulfate electrode (MSE) was selected as refer-ence electrode in all the electrochemical measurements,and a pure Pt foil as the counter electrode. Both PBSand the mixed solutions were purged with high purenitrogen (99.999%) for 30 min prior to measuring.Membrane electrode assembly (MEA) was prepared by

attaching NPG-Pt to carbon paper (TGP-H-060, Toray,Japan) first, and then hot-pressed onto one side of aNafion 115 membrane and commercial Pt/C (60 wt%,Johnson Matthey, UK) onto another side at 110°C and1.5 MPa for 195 s. As-prepared MEAs were thenassembled between high purity graphite plates as flow andcurrent collecting plates, which have single channel serpen-tine flow pattern. The anolyte was pumped to anode byperistaltic pump, while pure oxygen was fed to the cathodewithout humidification by a massflow controller. The celltemperature was controlled through a temperature control-ler and monitored by thermocouples buried in the graphiteblocks. The steady state polarization curves were recordedby automatic Electric Load (PLZ 70UA, Japan).

Preparation of NPG and NPG-Pt electrodesNPG was made by dealloying commercial 12-carat whitegold membrane in concentrated nitric acid for 20 minat 30°C [20]. Subsequently, NPG were immediatelytransferred to ultrapure water and repeatedly washed toremove Ag+ and NO3

-. NPG-Pt samples were preparedby floating the as-prepared NPG membranes at theinterface between the H2PtCl6 (1 g/L, pH = 10) solutionand the vapor of hydrazine hydrate (85%) in a closedsystem [22]. Deposition reaction occurred uniformlyon the surface of NPG. The amount of Pt depositedonto the NPG substrate gradually accumulates with

increasing plating time. The as-prepared NPG-Pt (load-ing of 0.1 mg cm-2 Au and 20 μg cm-2 Pt) samples weretransferred into ultrapure water as soon as the platingreaction finished. Then NPG-Pt membranes were affixedonto the clean GC electrode (4 mm in diameter) andfixed with 2 μL dilute nafion solution (0.5 wt%). The as-prepared NPG-Pt electrode was dried at room tempera-ture for 24 h before measurements.

Results and discussionSurface and crystal structure of the NPG-PtNPG-Pt samples were fabricated by chemical plating athin layer of Pt on NPG ligament surfaces. Figure 1a

Figure 1 Typical SEM (a) and TEM (b) images of the NPG-Pt 64sample.

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shows the wide scan SEM image of the as preparedNPG-Pt, which exhibits a three-dimensional continu-ous nanoporous structure, similar to the reported NPG[20]. Such structure is highly desirable in electrocataly-sis because of its structural integrity and electron con-ductivity. TEM observation (Figure 1b) clearly revealsthat for heavily plated samples, the deposited Pt formnanoislands uniformly coating on NPG surface. Pre-vious studies have proved that these Pt islands adopt aconformal and epitaxial relationship to the NPG sub-strate [24]. The amount and size of the Pt islands arecontrolled by varying the reaction time. According toICP-AES results, plating for 8 and 64 min (signed asNPG-Pt 8 and NPG-Pt 64, respectively) resulted in aPt loading of approximately 6 and 20 μg cm-2 in thefinal products, respectively.XRD was employed to investigate the crystalline

structure of NPG-Pt. Figure 2 shows XRD patternsfrom NPG and NPG-Pt samples which nearly exhibitthe same patterns. The diffraction peaks at 2θ = 38.4°,44.5° can be ascribed to the (111), (200) planes of face-centered cubic Au crystals respectively, with a lightlypositive shift relative to standard pattern. This com-mon positive shift of diffraction peaks are believed toresult from the strain in the nanoporous structure[26]. Interestingly, the (200) peak exhibits a muchhigher intensity than the theoretical value and evenexceeds the (111) peak, while (220) peak is nearly invi-sible in the patterns. These behaviors suggest that Ptplating does not affect the texture of the NPG mem-branes. Pt surface layer would not be able to exhibitits distinct diffractions due to its extremely low exist-ing amount.

Electrochemical characteristics of NPG-Pt in PBSThe NPG-Pt electrodes were further characterized bymeans of CV in 0.1 M PBS, as shown in Figure 3, whereNPG was also included for comparison. The fresh NPGexhibits an obvious anodic current rise at approximately0.4 V and a sharp cathodic peak at approximately0.05 V for Au surface oxides formation and reduction,respectively, similar to the reported polycrystalline Auelectrode in PBS [27]. After plating, it could be observedthat the well-defined hydrogen adsorption/desorptionpeaks in the potential region between ~ -1.0 and -0.7 Vshow up and gradually increase in intensity with theplating time. The Pt surface oxides formation begins atapproximately 0.2 V and the corresponding oxidesreduction peaks appear at approximately -0.42 V. Mean-while, the signals for gold surface oxides formation andreduction nearly disappear in the entire potential range,indicating a near complete coverage by the deposited Pt.These electrochemical characteristics of NPG-Pt are ingood agreement with previous observations in acid solu-tions [22].

Electrocatalytic properties of NPG-Pt for glucoseoxidation in neutral and alkaline solutionsThe electrocatalytic activity of NPG-Pt toward glucoseoxidation was evaluated by CV in PBS containing10 mM glucose, and a pure Pt electrode with smoothsurface was also included for comparison. As shown inFigure 4, all three samples show similar voltammetricbehavior in the presence of glucose, i.e., three main oxi-dation peaks (A1, A2, and A3) appear during the positivepotential scan at -0.84, -0.3, and 0.2 V, respectively,similar to the glucose oxidation on Pt-rich Au-Pt alloynanoparticles [4]. The peak A1 at the low potentialregion is often attributed to the dehydrogenation of

Figure 2 XRD patterns for NPG, NPG-Pt 8 and NPG-Pt 64samples.

Figure 3 CV curves for NPG and NPG-Pt 8, NPG-Pt 64 samplesin 0.1 M PBS, scan rate: 50 mV s-1. The currents were normalizedto the geometrical areas.

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glucose on active Pt surface, producing a layer ofadsorbed glucose intermediates on electrode surface [8].These intermediate species were then oxidized at a posi-tive potential, resulting in peaks A2 and A3. Furtherincreasing the potential, surface metal oxides generatewhich are nearly inactive for glucose oxidation, resultingin a current drop at higher potential. The peak A4 wasascribed to the glucose electroadsorption on the freshlyproduced active Pt surface at approximately -0.4 V dur-ing the negative scan. These voltammetric feathers arealso similar to other reported Pt-based bimetallic elec-trode, reflecting a similar reaction process. Meanwhile, itis observed that NPG-Pt samples exhibits substantiallyhigher peak current densities than Pt electrode, indicat-ing a superior catalytic activity toward glucose oxidation.In addition, NPG-Pt 64 exhibits the highest activityamong the three samples, due to the largest active surfacearea as revealed by CV in PBS in Figure 3. It is noted thatNPG-Pt membrane can directly be used as an unsup-ported electrocatalyst in PEM fuel cells [24,25]; therefore,these unique nanostructures can be expected to functionas active bimetallic anode catalysts in glucose fuel cells.In order to gain further insight into the surface struc-

ture effect of NPG-Pt on catalytic performance in glu-cose oxidation, the prolonged CV tests up to 800 cycleswere conducted on NPG-Pt 64 sample. In this electro-chemical process, the surface composite and structurewould be substantially changed by the repeated redox ofthe surface metal. This structure change was also foundto strongly affect the catalytic properties of NPG-Pt, asshown in Figure 5. While the peaks A1 and A3 graduallydecrease with the CV cycles, peak A2 obviously increasesin intensity and the onset potential also lightly shifts to

a negative value. According to the above discussion, theloss of active Pt surface, resulting from the surface Ptalloying with the NPG substrate during the CV process,would be responsible for the corresponding peakdecrease for A1 and A3. Meanwhile, the peak A2 expan-sion suggests that the new surface from CV process ismore active for the intermediate species. This is not sur-prised since Au is active for glucose oxidation at thispotential in PBS [27]. Therefore, we could improve thecatalytic performance of NPG-Pt by tailoring the surfacestructure to maintain the catalytic activity at low poten-tial and enhance the ability of oxidizing the adsorbedintermediate species (because these intermediate canhinder the glucose adsorption on Pt surface).Figure 6 shows the CV curves of NPG-Pt in the mixed

solution of NaOH and 10 mM glucose. As in PBS, threeoxidation peaks were observed in the positive scan, indi-cating a similar reaction process. Nevertheless, theobserved high current densities as compared to that inPBS suggest that glucose oxidation in alkaline solutionproceeds more rapidly than in neutral solution, due tothe high concentration of OH- ions which are believedto be directly involved in the reaction intermediates oxi-dation [6]. This is also in agreement with previousobservation that Pt-decorated NPG could exhibit highactivity and good stability for methanol oxidation inalkaline solution [21]. Again, the NPG-Pt 64 sampleexhibits the highest activity, with a peak current densityapproximately 1.5 and 3.4 mA cm-2 for peaks A1 andA2, respectively, which are about seven times higherthan those on pure Pt electrode.

DGFCs in neutral and alkaline solutionFigure 7 shows typical polarization curves of DGFC withNPG-Pt 64 working as anode and commercial Pt/C as

Figure 4 CV curves obtained for NPG-Pt 8 and NPG-Pt 64samples in a mixed solution of 0.1 M PBS + 10 mM glucose,scan rate: 50 mV s-1. Pure Pt electrode was included forcomparison and the currents were normalized to the geometricalareas.

Figure 5 Prolonged CV curves of NPG-Pt 64 electrode in PBScontaining10 mM glucose, scan rate: 50 mV s-1. The currentswere normalized to the geometrical areas.

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cathode catalyst, and Nafion 115 membrane as electro-lyte at 40 and 60°C in neutral and alkaline solutions.The loading of the catalyst were 0.3 mg cm-2 Au and60 μg cm-2 Pt which are three times as much as those inprevious experiment. The OCVs (Figure 7a) were almostthe same (~0.8 V) at 40 and 60°C and their maximumpower densities were 0.14 and 0.18 mW cm-2, which wasmuch higher than the one reported [28]. In alkaline con-dition (Figure 7b), the OCVs were almost the same too(~0.9 V) at 40 and 60°C and accordingly their maximumpower densities were 2.5 and 4.4 mW cm-2, which exceedthe reported data [29,30]. By maintaining the concentra-tion of glucose at 0.5 M in 0.1 M PBS and 2 M NaOHrespectively, it can be observed that both in neutral andalkaline solutions, the cell performance increased withtemperature, which would be due to the faster electro-chemical kinetics of both the anodic and cathodic reac-tions, increased conductivity of the electrolyte andenhanced diffusion rate of glucose and oxygen.It also can be seen that the maximum power densities

in alkaline (Figure 7b) was 4.4 mW cm-2 which is about24 times than that in neutral solution (0.18 mW cm-2,Figure 7a). This should be mainly attributed to quickerreaction rate on the NPG-Pt in alkaline than that inneutral solution for glucose oxidation which was in linewith the results of 3.3 above.

ConclusionsNPG-Pt membranes, a type of porous Au-Pt bimetallicnanostructures, were fabricated by chemically platingthin layer of Pt on NPG and were studied for glucoseelectrooxidation and the application in fuel cell. Takingadvantage of the unique structure and high surface

area, NPG-Pt exhibits considerable activity toward thisreaction in neutral and alkaline solutions. In addition,glucose oxidation on NPG-Pt was found to be a sur-face sensitive process and Au-Pt surface alloy is highlyactive for oxidizing the adsorbed intermediate speciesresulted from the glucose electroadsorption. Thismeans we could further improve the catalytic perfor-mance of NPG-Pt by tailoring the surface compositeand structure. The results of DGFC test indicated thatNPG-Pt is expected as a promising low precious metalloading electrocatalyst for application in glucosefuel cells.

AbbreviationsCV: cyclic voltammetry; DGFC: direct glucose fuel cell; ICP-AES: inductivelycoupled plasma-atomic emission spectrometry; MEA: membrane electrodeassembly; MSE: mercury sulfate electrode; NPG: nanoporous gold; NPG-Pt: Pt-decorated nanoporous gold; SEM: scanning electron microscopy; TEM:transmission electron microscopy; XRD: X-ray powder diffraction.

AcknowledgementsThis work was supported by the Ph.D. Programs Foundation of the MOE(20090131110019). We thank Prof. Y. Ding and HouYi Ma for valuablediscussions and for sharing their nanomaterials and facilities.

Figure 6 CV curves for NPG-Pt 8 and NPG-Pt 64 samples in amixed solution of 0.1 M NaOH + 10 mM glucose, scan rate:50 mV s-1. Pure Pt electrode was included for comparison and thecurrents were normalized to the geometrical areas.

Figure 7 Performance of DGFC at various temperatures in0.1 M PBS containing 0.5 M glucose (a) and in 2 M NaOHcontaining 0.5 M glucose (b) with NPG-Pt 64 as the catalyst foranode and commercial Pt/C as cathode. The flow rates of theanolyte and the air are 2 and 120 mL min-1, respectively.

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Author details1School of Chemistry and Chemical Engineering, Shandong University, Jinan250100, China. 2School of Chemistry and Bioscience, Ili Normal University,Xinjiang 835000, China.

Authors’ contributionsSongzhi Cui carried out the electrochemical measurements and drafted themanuscript. Xinbo Ge carried out the XRD studies, participated in thesequence alignment and revised the manuscript. Xiuling yan conceived ofthe study, and participated in its design and performed the fuel cell tests. Allauthors read and approved the final manuscript.

Competing interestsThe authors declare that they have no competing interests.

Received: 1 February 2011 Accepted: 7 April 2011Published: 7 April 2011

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doi:10.1186/1556-276X-6-313Cite this article as: Yan et al.: Pt-decorated nanoporous gold for glucoseelectrooxidation in neutral and alkaline solutions. Nanoscale ResearchLetters 2011 6:313.

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